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Synthetic method of perfluoroisobutyronitrile
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A technology of perfluoroisobutyronitrile and a synthesis method is applied in the field of synthesis of perfluoroisobutyronitrile, and can solve problems such as increased production cost, environmental pollution, long route and the like
Pending Publication Date: 2020-10-27
福建省漳平市九鼎氟化工有限公司
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Although this technical route is mature and reliable, there is a long route, and the involved chemicals such as d
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Embodiment 1
[0060] A kind of synthetic method of the perfluoroisobutyronitrile of the embodiment of the present invention, its synthetic scheme is as follows figure 1 Shown, this synthesis method comprises the following steps:
[0061] (1) Synthesis of oxalyl fluoride monoester
[0062] First, the reaction system is heated and vacuumized to remove water, and the whole system is purged with high-purity nitrogen to remove oxygen therein; the reactor is cooled to normal temperature, and under the protection of nitrogen, tetraethylene glycol dimethyl ether (444.6g) is passed into the reactor. , 2mol), add dry potassium fluoride (29.0g, 0.5mol), add monoethyl oxalyl chloride (272.9g, 2mol) and stir; heat up to 130 ° C, keep the temperature for 5 hours; separate the fluorocarbon layer after the reaction , Distilled under reduced pressure to obtain monoethyl oxalyl fluoride (232.1 g, 1.94 mol) with a yield of 97%.
[0063] (2) Synthesis of ethyl heptafluoro-2-carbonyl-3-methylbutyrate
[006...
Embodiment 2
[0072] A kind of synthetic method of the perfluoroisobutyronitrile of the embodiment of the present invention, its synthetic scheme is as follows figure 2 Shown, this synthesis method comprises the following steps:
[0073] (1) Synthesis of oxalyl fluoride monoester
[0074] First, the reaction system is heated and vacuumized to remove water, and the whole system is purged with high-purity nitrogen to remove oxygen therein; the reactor is cooled to normal temperature, and under the protection of nitrogen, tetraethylene glycol dimethyl ether (444.6g) is passed into the reactor. , 2mol), add dry potassium fluoride (29.0g, 0.5mol), add monoethyl oxalyl chloride (272.9g, 2mol) and stir; heat up to 130 ° C, keep the temperature for 5 hours; separate the fluorocarbon layer after the reaction , Distilled under reduced pressure to obtain monoethyl oxalyl fluoride (232.1 g, 1.94 mol) with a yield of 97%.
[0075] (2) Synthesis of ethyl heptafluoro-2-carbonyl-3-methylbutyrate
[007...
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Abstract
The invention discloses a synthesis method of perfluoroisobutyronitrile, comprising the following steps of: (1) carrying out a reaction between oxalyl chloride monoester and fluoride salt in a solventto obtain oxalyl fluoride monoester; (2) carrying out a reaction between oxalyl fluoride monoester and hexafluoropropylene in a solvent by taking fluoride salt as a catalyst to prepare heptafluoro-2-carbonyl-3-methylbutyrate; (3) carrying out catalytic decarbonylation on heptafluoro-2-carbonyl-3-methylbutyrate in a solvent through cesium fluoride, so as to obtain heptafluoroisobutyrate; and (4) carrying out a reaction between heptafluoroisobutyrate and ammonia, and dehydrating to obtain perfluoroisobutyronitrile. The synthetic method has the advantages of easily available raw materials, mildreaction conditions, high raw material conversion rate and product yield, safe and simple process operation, and easy realization of industrial production.
Description
technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing perfluoroisobutyronitrile. Background technique [0002] Heptafluoroisobutyronitrile (perfluoroisobutyronitrile), namely 2,3,3,3-tetrafluoro-2-trifluoromethylpropionitrile, is a class of perfluoronitrile compounds with a boiling point of -4.7°C. It is a colorless gas at normal temperature and pressure. It has the characteristics of low boiling point, high volatility, excellent electrical insulation properties and good environmental protection performance, and can be used as a gas dielectric material and a dielectric composition for insulators in electrical devices. The greenhouse effect index (GWP) of heptafluoroisobutyronitrile is only 2210, which is much lower than that of sulfur hexafluoride (GWP=23500). It can be used to replace the traditional sulfur hexafluoride insulating gas and greatly reduce the problem of atmospheric greenhouse effe...
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